CN108226245B - Test method for corrosion resistance of 304 stainless steel under high temperature conditions - Google Patents
Test method for corrosion resistance of 304 stainless steel under high temperature conditions Download PDFInfo
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- 239000010963 304 stainless steel Substances 0.000 title claims abstract description 21
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 title claims abstract description 21
- 238000005260 corrosion Methods 0.000 title claims abstract description 21
- 230000007797 corrosion Effects 0.000 title claims abstract description 21
- 238000010998 test method Methods 0.000 title 1
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 99
- 239000010959 steel Substances 0.000 claims abstract description 99
- 239000000919 ceramic Substances 0.000 claims abstract description 30
- 238000007789 sealing Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 15
- 239000000084 colloidal system Substances 0.000 claims description 12
- 239000004744 fabric Substances 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- 238000013461 design Methods 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical group [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 3
- 239000003365 glass fiber Substances 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 2
- 230000007423 decrease Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 17
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 6
- 238000007654 immersion Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000002848 electrochemical method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
本发明公开了高温条件下304不锈钢耐腐蚀性能的检测方法，其方法为将电极系统安装于高温高压反应釜中，利用Autolab302N电化学工作站测定304不锈钢在1500ppmH3BO3+2.3ppmLiOH的水溶液中的电化学噪声谱，所述电极系统系统包括工作电极装置和参比‑对电极装置；工作电极装置的上端设置上螺扣结构，下端设置下螺扣结构，在钢管的内部设置有接线杆，在钢管上一次设置有第一螺帽，第二螺帽和第三螺帽，在接线杆下端连接工作电极试样，参比‑对电极装置内部设置参比电极和对电极，在钢管内部从上至下依次设置上绝缘层，上密封层，双孔陶瓷片，下密封层和下绝缘层，在钢管上端设置上紧固螺母，在钢管下端设置下紧固螺母；在25‑250℃条件下，304不锈钢的耐腐蚀性能随温度升高不断降低。
The invention discloses a method for detecting the corrosion resistance of 304 stainless steel under high temperature conditions. The method is to install an electrode system in a high temperature and high pressure reaction kettle, and use an Autolab302N electrochemical workstation to measure the electrochemical noise of 304 stainless steel in an aqueous solution of 1500ppmH3BO3+2.3ppmLiOH The electrode system system includes a working electrode device and a reference-counter electrode device; the upper end of the working electrode device is provided with an upper screw structure, the lower end is provided with a lower screw structure, and a terminal rod is arranged inside the steel pipe. A first nut, a second nut and a third nut are provided, and the working electrode sample is connected to the lower end of the terminal rod. The reference-counter electrode device is provided with a reference electrode and a counter electrode, which are arranged from top to bottom inside the steel pipe. Set the upper insulating layer, the upper sealing layer, the double-hole ceramic sheet, the lower sealing layer and the lower insulating layer, set the upper tightening nut on the upper end of the steel pipe, and set the lower tightening nut on the lower end of the steel pipe; under the condition of 25-250℃, 304 stainless steel The corrosion resistance decreases with increasing temperature.
Description
本发明申请是母案申请“一种用于高温高压水环境中电化学测量的电极系统及其应用”的分案申请，母案申请的申请日为2016年7月22日，母案申请的申请号为2016105993363。The present application is a divisional application of the parent application "An Electrode System for Electrochemical Measurement in High Temperature and High Pressure Water Environment and Its Application". The filing date of the parent application is July 22, 2016, and the parent application The application number is 2016105993363.
技术领域technical field
本发明属于电化学电极材料技术领域，尤其是高温条件下304不锈钢耐腐蚀性能的检测方法。The invention belongs to the technical field of electrochemical electrode materials, in particular to a method for detecting the corrosion resistance of 304 stainless steel under high temperature conditions.
背景技术Background technique
能够耐高温高压、耐腐蚀的特种传感器，是一种包括先进的高温材料学、精密机械加工、电子学、精细化学等多种高新科学技术的高技术产品。这种能在高温高压和强腐蚀的严酷环境中工作的传感器，生产难度极大。由于国内在研制此类传感器关键的技术方面一直没有进展，因此多年来几乎全部依赖进口。而在石油、化工、核能等领域中，有很多重要的工艺必须在高温高压和强腐蚀环境中实施。The special sensor that can withstand high temperature and high pressure and corrosion resistance is a high-tech product including advanced high-temperature material science, precision machining, electronics, fine chemistry and other high-tech science and technology. This kind of sensor, which can work in the harsh environment of high temperature, high pressure and strong corrosion, is extremely difficult to produce. Since there has been no progress in the development of key technologies for such sensors in China, almost all of them have relied on imports for many years. In the fields of petroleum, chemical, nuclear energy, etc., there are many important processes that must be implemented in high temperature, high pressure and strong corrosive environments.
发明内容SUMMARY OF THE INVENTION
本发明克服了现有技术中的缺点，提供了一种用于高温高压水环境中电化学测量的电极系统及其应用。The invention overcomes the shortcomings of the prior art, and provides an electrode system for electrochemical measurement in a high temperature and high pressure water environment and its application.
为了解决上述技术问题，本发明是通过以下技术方案实现的：In order to solve the above-mentioned technical problems, the present invention is achieved through the following technical solutions:
一种用于304不锈钢耐腐蚀性能检测的电极系统，包括工作电极装置和参比-对电极装置；An electrode system for the detection of corrosion resistance of 304 stainless steel, including a working electrode device and a reference-counter electrode device;
工作电极装置的主体为一钢管，钢管的上端设置上螺扣结构，下端设置下螺扣结构，用于与螺帽配合固定接线杆，钢管内部中空，在钢管的内部设置有接线杆，接线杆的两端伸出钢管，在接线杆的上方伸出钢管的位置设置上套管，在接线杆的下方伸出钢管的位置设置下套管，上套管和下套管均卡在接线杆与钢管之间，用于固定和密封，接线杆位于钢管内的整个部分包裹一层绝缘布，在钢管的上螺扣结构的上端设置有第一螺帽，第一螺帽套在接线杆上，与上螺扣结构通过螺纹连接，下螺扣结构与钢管连接处设置有卡箍和第二螺帽，卡箍垫在下螺扣结构与钢管之间，第二螺帽与下螺扣结构通过螺纹连接，下螺扣结构的下端设置有第三螺帽，第三螺帽的下端设置有锥形凹槽，接线杆伸出第三螺帽的部分上连接工作电极试样，在工作电极试样与第三螺帽连接处设置有锥形套管；The main body of the working electrode device is a steel pipe. The upper end of the steel pipe is provided with an upper screw structure, and the lower end is provided with a lower screw structure, which is used to cooperate with the nut to fix the terminal rod. The interior of the steel pipe is hollow. The two ends protrude from the steel pipe, the upper casing is set at the position where the steel pipe protrudes above the connecting rod, and the lower casing is set at the position where the steel pipe extends below the connecting rod. Between the steel pipes, it is used for fixing and sealing. The entire part of the terminal rod located in the steel pipe is wrapped with a layer of insulating cloth. The upper end of the upper screw structure of the steel pipe is provided with a first nut, and the first nut is sleeved on the terminal rod. It is connected with the upper screw structure by threads, and the connection between the lower screw structure and the steel pipe is provided with a clamp and a second nut, the clamp is cushioned between the lower screw structure and the steel pipe, and the second nut and the lower screw structure are connected by threads Connection, the lower end of the lower screw structure is provided with a third nut, the lower end of the third nut is provided with a conical groove, the part of the terminal rod extending out of the third nut is connected to the working electrode sample, and the working electrode sample is connected to the working electrode sample. A conical sleeve is arranged at the connection with the third nut;
在上述技术方案中，工作电极装置的钢管为316L不锈钢，钢管的内径为2.5-3.5mm，外径为6-8mm，长度为150-250mm。In the above technical solution, the steel pipe of the working electrode device is 316L stainless steel, the inner diameter of the steel pipe is 2.5-3.5 mm, the outer diameter is 6-8 mm, and the length is 150-250 mm.
在上述技术方案中，接线杆为316L不锈钢，直径为2-5mm，长度为250-350mm。In the above technical solution, the terminal rod is made of 316L stainless steel, with a diameter of 2-5mm and a length of 250-350mm.
在上述技术方案中，绝缘布为玻璃纤维绝缘布。In the above technical solution, the insulating cloth is glass fiber insulating cloth.
参比-对电极装置的外层为钢管，钢管内部中空，在钢管内部设置参比电极和对电极，参比电极与参比电极连接导线相连，参比电极上端伸出钢管上沿，参比电极连接导线下端伸出钢管下沿，对电极与对电极连接导线相连，对电极上端伸出钢管上沿，对电极连接导线下端伸出钢管下沿，参比电极及其连接导线、对电极及其连接导线与钢管外壁平行设置，互相不接触，在钢管内部从上至下依次设置上绝缘层，上密封层，双孔陶瓷片，下密封层和下绝缘层，在钢管上端设置上紧固螺母，在钢管下端设置下紧固螺母；The outer layer of the reference-counter electrode device is a steel pipe, the inside of the steel pipe is hollow, and the reference electrode and the counter electrode are arranged inside the steel pipe. The lower end of the electrode connection wire protrudes from the lower edge of the steel pipe, the counter electrode is connected to the counter electrode connection wire, the upper end of the counter electrode protrudes from the upper edge of the steel pipe, the lower end of the counter electrode connection wire protrudes from the lower edge of the steel pipe, the reference electrode and its connecting wire, the counter electrode and the The connecting wires are arranged in parallel with the outer wall of the steel pipe and do not contact each other. The upper insulating layer, the upper sealing layer, the double-hole ceramic sheet, the lower sealing layer and the lower insulating layer are sequentially arranged inside the steel pipe from top to bottom. Nut, tighten the nut under the lower end of the steel pipe;
在上述技术方案中，所述的参比-对电极装置的钢管为316L不锈钢管，钢管的内径为8-10mm，外径为12-14mm，长度为350-450mm。In the above technical solution, the steel pipe of the reference-counter electrode device is a 316L stainless steel pipe, the inner diameter of the steel pipe is 8-10mm, the outer diameter is 12-14mm, and the length is 350-450mm.
在上述技术方案中，所述的双孔陶瓷片的数量为8-15片，双孔陶瓷片的厚度为1-2cm。In the above technical solution, the number of the bi-porous ceramic sheets is 8-15, and the thickness of the bi-porous ceramic sheets is 1-2 cm.
在上述技术方案中，所述的参比电极为氯化银丝，对电极为铂片。In the above technical solution, the reference electrode is a silver chloride wire, and the counter electrode is a platinum sheet.
在上述技术方案中，所述的上绝缘层为聚四氟乙烯层，所述的下绝缘层为聚四氟乙烯层。In the above technical solution, the upper insulating layer is a polytetrafluoroethylene layer, and the lower insulating layer is a polytetrafluoroethylene layer.
在上述技术方案中，所述的上密封层为陶瓷粉胶体层，所述的下密封层为陶瓷粉胶体层。In the above technical solution, the upper sealing layer is a ceramic powder colloid layer, and the lower sealing layer is a ceramic powder colloid layer.
一种用于304不锈钢耐腐蚀性能检测的电极系统的制备方法，按照下列步骤进行：A preparation method of an electrode system for detecting the corrosion resistance of 304 stainless steel is carried out according to the following steps:
步骤1：按照工作电极装置的结构组装工作电极；Step 1: Assemble the working electrode according to the structure of the working electrode device;
步骤2：将参比电极及其连接导线和对电极及其连接导线，放入钢管内部，保持彼此不接触；Step 2: Put the reference electrode and its connecting wire, and the counter electrode and its connecting wire into the steel pipe and keep them out of contact with each other;
步骤3：将8-15片双孔陶瓷片套在参比电极和对电极上，卡在钢管内壁上，使双孔陶瓷片位于钢管管体的中部位置；Step 3: Put 8-15 double-hole ceramic sheets on the reference electrode and the counter electrode, and clamp them on the inner wall of the steel pipe, so that the double-hole ceramic sheet is located in the middle of the steel pipe body;
步骤4：将陶瓷粉与水按照质量比(3-5)：1的比例混匀搅拌，从钢管的上方与下方倒入钢管中，形成一定厚度的陶瓷粉胶体层；Step 4: Mix and stir the ceramic powder and water according to the mass ratio (3-5): 1, and pour it into the steel pipe from the top and bottom of the steel pipe to form a ceramic powder colloid layer of a certain thickness;
步骤5：将聚四氟柱体从钢管上方和下方塞入参比电极、对电极与钢管内壁的空隙中，压住陶瓷粉胶体层，保持密封；Step 5: Insert the PTFE cylinder from the top and bottom of the steel pipe into the gap between the reference electrode, the counter electrode and the inner wall of the steel pipe, press the ceramic powder colloid layer, and keep it sealed;
步骤6：在钢管的上端拧紧上紧固螺母，在钢管的下端拧紧下紧固螺母，将整个装置在室温(20-25摄氏度)下静置20-30小时，使陶瓷粉胶体凝固。Step 6: Tighten the upper tightening nut on the upper end of the steel pipe, tighten the lower tightening nut on the lower end of the steel pipe, and let the whole device stand at room temperature (20-25 degrees Celsius) for 20-30 hours to solidify the ceramic powder colloid.
与现有技术相比，本发明的有益效果是：本发明适合实验室使用，能够模拟核电站高温高压条件下电化学测量的环境，工作环境最高温度范围约为160℃～250℃，最高压力范围约为6MPa～10MPa，本装置有较好的密封性，能满足绝缘要求，并且制备简单、稳定性好、使用便捷。Compared with the prior art, the beneficial effects of the present invention are: the present invention is suitable for laboratory use, can simulate the environment of electrochemical measurement under high temperature and high pressure conditions of nuclear power plants, the maximum temperature range of the working environment is about 160°C to 250°C, and the maximum pressure range is about 160°C to 250°C. About 6MPa-10MPa, the device has good sealing performance, can meet the insulation requirements, and is simple in preparation, good in stability and convenient in use.
附图说明Description of drawings
图1为本发明中工作电极装置结构示意图(图示左侧为上方)。FIG. 1 is a schematic structural diagram of the working electrode device in the present invention (the left side of the figure is the top).
图2为本发明中参比-对电极装置结构示意图。FIG. 2 is a schematic structural diagram of the reference-counter electrode device in the present invention.
图3为实施例示图1。FIG. 3 is an example of FIG. 1 .
图4为实施例示图2。FIG. 4 is an example of FIG. 2 .
图5为实施例示图3。FIG. 5 is an example of FIG. 3 .
其中，1为上套管，2为第一螺帽，3为上螺扣结构，4为钢管，5为接线杆，6为第二螺帽，7为卡箍，8为下螺扣结构，9为下套管，10为第三螺帽，11为锥形套管，12为工作电极试样，13为参比电极，14为对电极，15为上紧固螺母，16为上绝缘层，17为上密封层，18为参比电极连接导线，19为对电极连接导线，20为双孔陶瓷片，21为下密封层，22为下绝缘层，23为下紧固螺母。Among them, 1 is the upper casing, 2 is the first nut, 3 is the upper screw structure, 4 is the steel pipe, 5 is the connecting rod, 6 is the second nut, 7 is the clamp, 8 is the lower screw structure, 9 is the lower casing, 10 is the third nut, 11 is the conical casing, 12 is the working electrode sample, 13 is the reference electrode, 14 is the counter electrode, 15 is the upper fastening nut, and 16 is the upper insulating layer , 17 is the upper sealing layer, 18 is the reference electrode connecting wire, 19 is the opposite electrode connecting wire, 20 is the double-hole ceramic sheet, 21 is the lower sealing layer, 22 is the lower insulating layer, and 23 is the lower fastening nut.
具体实施方式Detailed ways
下面结合附图与具体的实施方式对本发明作进一步详细描述：The present invention is described in further detail below in conjunction with the accompanying drawings and specific embodiments:
一种用于304不锈钢耐腐蚀性能检测的电极系统，包括工作电极装置和参比-对电极装置；An electrode system for the detection of corrosion resistance of 304 stainless steel, including a working electrode device and a reference-counter electrode device;
工作电极装置的主体为一钢管，钢管的上端设置上螺扣结构，下端设置下螺扣结构，用于与螺帽配合固定接线杆，钢管内部中空，在钢管的内部设置有接线杆，接线杆的两端伸出钢管，在接线杆的上方伸出钢管的位置设置上套管，在接线杆的下方伸出钢管的位置设置下套管，上套管和下套管均卡在接线杆与钢管之间，用于固定和密封，接线杆位于钢管内的整个部分包裹一层绝缘布，在钢管的上螺扣结构的上端设置有第一螺帽，第一螺帽套在接线杆上，与上螺扣结构通过螺纹连接，下螺扣结构与钢管连接处设置有卡箍和第二螺帽，卡箍垫在下螺扣结构与钢管之间，第二螺帽与下螺扣结构通过螺纹连接，下螺扣结构的下端设置有第三螺帽，第三螺帽的下端设置有锥形凹槽，接线杆伸出第三螺帽的部分上连接工作电极试样，在工作电极试样与第三螺帽连接处设置有锥形套管；The main body of the working electrode device is a steel pipe. The upper end of the steel pipe is provided with an upper screw structure, and the lower end is provided with a lower screw structure, which is used to cooperate with the nut to fix the terminal rod. The interior of the steel pipe is hollow. The two ends protrude from the steel pipe, the upper casing is set at the position where the steel pipe protrudes above the connecting rod, and the lower casing is set at the position where the steel pipe extends below the connecting rod. Between the steel pipes, it is used for fixing and sealing. The entire part of the terminal rod located in the steel pipe is wrapped with a layer of insulating cloth. The upper end of the upper screw structure of the steel pipe is provided with a first nut, and the first nut is sleeved on the terminal rod. It is connected with the upper screw structure by threads, and the connection between the lower screw structure and the steel pipe is provided with a clamp and a second nut, the clamp is cushioned between the lower screw structure and the steel pipe, and the second nut and the lower screw structure are connected by threads Connection, the lower end of the lower screw structure is provided with a third nut, the lower end of the third nut is provided with a conical groove, the part of the terminal rod extending out of the third nut is connected to the working electrode sample, and the working electrode sample is connected to the working electrode sample. A conical sleeve is arranged at the connection with the third nut;
在上述技术方案中，工作电极装置的钢管为316L不锈钢，钢管的内径为2.5-3.5mm，外径为6-8mm，长度为150-250mm。In the above technical solution, the steel pipe of the working electrode device is 316L stainless steel, the inner diameter of the steel pipe is 2.5-3.5 mm, the outer diameter is 6-8 mm, and the length is 150-250 mm.
在上述技术方案中，接线杆为316L不锈钢，直径为2-5mm，长度为250-350mm。In the above technical solution, the terminal rod is made of 316L stainless steel, with a diameter of 2-5mm and a length of 250-350mm.
在上述技术方案中，绝缘布为玻璃纤维绝缘布。In the above technical solution, the insulating cloth is glass fiber insulating cloth.
参比-对电极装置的外层为钢管，钢管内部中空，在钢管内部设置参比电极和对电极，参比电极与参比电极连接导线相连，参比电极上端伸出钢管上沿，参比电极连接导线下端伸出钢管下沿，对电极与对电极连接导线相连，对电极上端伸出钢管上沿，对电极连接导线下端伸出钢管下沿，参比电极及其连接导线、对电极及其连接导线与钢管外壁平行设置，互相不接触，在钢管内部从上至下依次设置上绝缘层，上密封层，双孔陶瓷片，下密封层和下绝缘层，在钢管上端设置上紧固螺母，在钢管下端设置下紧固螺母；The outer layer of the reference-counter electrode device is a steel pipe, the inside of the steel pipe is hollow, and the reference electrode and the counter electrode are arranged inside the steel pipe. The lower end of the electrode connection wire protrudes from the lower edge of the steel pipe, the counter electrode is connected to the counter electrode connection wire, the upper end of the counter electrode protrudes from the upper edge of the steel pipe, the lower end of the counter electrode connection wire protrudes from the lower edge of the steel pipe, the reference electrode and its connecting wire, the counter electrode and the The connecting wires are arranged in parallel with the outer wall of the steel pipe and do not contact each other. The upper insulating layer, the upper sealing layer, the double-hole ceramic sheet, the lower sealing layer and the lower insulating layer are sequentially arranged inside the steel pipe from top to bottom. Nut, tighten the nut under the lower end of the steel pipe;
在上述技术方案中，所述的参比-对电极装置的钢管为316L不锈钢管，钢管的内径为8-10mm，外径为12-14mm，长度为350-450mm。In the above technical solution, the steel pipe of the reference-counter electrode device is a 316L stainless steel pipe, the inner diameter of the steel pipe is 8-10mm, the outer diameter is 12-14mm, and the length is 350-450mm.
在上述技术方案中，所述的双孔陶瓷片的数量为8-15片，双孔陶瓷片的厚度为1-2cm。In the above technical solution, the number of the bi-porous ceramic sheets is 8-15, and the thickness of the bi-porous ceramic sheets is 1-2 cm.
在上述技术方案中，所述的参比电极为氯化银丝，对电极为铂片。In the above technical solution, the reference electrode is a silver chloride wire, and the counter electrode is a platinum sheet.
在上述技术方案中，所述的上绝缘层为聚四氟乙烯层，所述的下绝缘层为聚四氟乙烯层。In the above technical solution, the upper insulating layer is a polytetrafluoroethylene layer, and the lower insulating layer is a polytetrafluoroethylene layer.
在上述技术方案中，所述的上密封层内设置陶瓷粉胶体层，所述的下密封层内设置陶瓷粉胶体层。In the above technical solution, a ceramic powder colloid layer is arranged in the upper sealing layer, and a ceramic powder colloid layer is arranged in the lower sealing layer.
参比-对电极装置的制备方法，制备时，陶瓷粉选用美国Cotronics公司研制的Duropot809系列，氯化银丝和铂片选用天津艾达恒晟科技发展有限公司的产品，按照下列步骤进行：For the preparation method of the reference-counter electrode device, during preparation, the ceramic powder is selected from the Duropot809 series developed by Cotronics Company in the United States, and the silver chloride wire and platinum sheet are selected from the products of Tianjin Aida Hengsheng Technology Development Co., Ltd., according to the following steps:
步骤1：按照工作电极装置的结构组装工作电极；Step 1: Assemble the working electrode according to the structure of the working electrode device;
步骤2：将参比电极及其连接导线和对电极及其连接导线，放入钢管内部，保持彼此不接触；Step 2: Put the reference electrode and its connecting wire, and the counter electrode and its connecting wire into the steel pipe and keep them out of contact with each other;
步骤3：将8-15片双孔陶瓷片套在参比电极和对电极上，卡在钢管内壁上，使双孔陶瓷片位于钢管管体的中部位置；Step 3: Put 8-15 double-hole ceramic sheets on the reference electrode and the counter electrode, and clamp them on the inner wall of the steel pipe, so that the double-hole ceramic sheet is located in the middle of the steel pipe body;
步骤4：将陶瓷粉与水按照质量比(3-5)：1的比例混匀搅拌，从钢管的上方与下方倒入钢管中，形成一定厚度的陶瓷粉胶体层；Step 4: Mix and stir the ceramic powder and water according to the mass ratio (3-5): 1, and pour it into the steel pipe from the top and bottom of the steel pipe to form a ceramic powder colloid layer of a certain thickness;
步骤5：将聚四氟柱体从钢管上方和下方塞入参比电极、对电极与钢管内壁的空隙中，压住陶瓷粉胶体层，保持密封；Step 5: Insert the PTFE cylinder from the top and bottom of the steel pipe into the gap between the reference electrode, the counter electrode and the inner wall of the steel pipe, press the ceramic powder colloid layer, and keep it sealed;
步骤6：在钢管的上端拧紧上紧固螺母，在钢管的下端拧紧下紧固螺母，将整个装置在室温(20-25摄氏度)下静置20-30小时，使陶瓷粉胶体凝固。Step 6: Tighten the upper tightening nut on the upper end of the steel pipe, tighten the lower tightening nut on the lower end of the steel pipe, and let the whole device stand at room temperature (20-25 degrees Celsius) for 20-30 hours to solidify the ceramic powder colloid.
以下通过具体测试实施例进行说明：Described below through specific test examples:
将研制出的电极测量系统安装于高温高压反应釜(设计温度350℃、设计压力25MPa)中，利用Autolab302N电化学工作站测定了不同温度、浸泡时间下304不锈钢在1500ppmH3BO3+2.3ppmLiOH的水溶液中的电化学噪声谱。图3是304不锈钢在1500ppmH3BO3+2.3ppmLiOH的水溶液常温浸泡实验中噪声电阻随时间的变化，可以看出随着浸泡时间的延长噪声电阻值趋于下降；第二天后噪声电阻又有增大的趋势，是由于浸泡初期发生均匀腐蚀，随着浸泡时间的延长表面生成了氧化膜导致噪声电阻又逐渐增大。图4是不同温度下304不锈钢在1500ppmH3BO3+2.3ppmLiOH的水溶液的噪声电阻随时间的变化关系，可以看出随着温度从25-250℃的升高304不锈钢的耐腐蚀性不断降低。The developed electrode measurement system was installed in a high temperature and high pressure reactor (design temperature 350℃, design pressure 25MPa), and the aqueous solution of 304 stainless steel in 1500ppmH 3 BO 3 +2.3ppm LiOH was measured at different temperatures and immersion times by using Autolab302N electrochemical workstation. Electrochemical noise spectrum in . Figure 3 shows the change of noise resistance with time in the immersion experiment of 304 stainless steel in 1500ppmH 3 BO 3 +2.3ppm LiOH aqueous solution at room temperature. It can be seen that the noise resistance value tends to decrease with the prolongation of immersion time; after the second day, the noise resistance increases again. The big trend is due to uniform corrosion at the initial stage of immersion, and as the immersion time prolongs, an oxide film is formed on the surface, resulting in a gradual increase in noise resistance. Figure 4 shows the relationship between the noise resistance of 304 stainless steel in an aqueous solution of 1500ppmH 3 BO 3 + 2.3ppm LiOH at different temperatures with time. It can be seen that the corrosion resistance of 304 stainless steel decreases with the increase of temperature from 25-250 ℃.
如图5所示，将研制出的电极测量系统安装于高温高压反应釜(设计温度350℃、设计压力25MPa)中，利用Autolab302N电化学工作站测定了不同压力下X65管线钢在3.5％wt.NaCl的水溶液中的极化曲线。经计算可得在压力分别为5MPa、10MPa和17MPa时，腐蚀电流密度分别为2.323×10-5A·cm-2、3.407×10-5A·cm-2和8.723×10-5A·cm-2。腐蚀电流密度随压力增大而增大，说明X65管线钢随压力的增高腐蚀速率加快。As shown in Figure 5, the developed electrode measurement system was installed in a high-temperature and high-pressure reactor (design temperature 350 °C, design pressure 25 MPa), and the Autolab302N electrochemical workstation was used to measure the 3.5% wt.NaCl of X65 pipeline steel under different pressures. Polarization curves in aqueous solutions. The calculated corrosion current densities are 2.323×10 -5 A·cm -2 , 3.407×10 -5 A·cm -2 and 8.723×10 -5 A·cm -2 when the pressures are 5MPa, 10MPa and 17MPa, respectively. -2 . The corrosion current density increases with the increase of pressure, indicating that the corrosion rate of X65 pipeline steel increases with the increase of pressure.
根据以上实施例说明本发明的电极系统真实反映出了电化学的性能变化，说明本装置在高温(针对304不锈钢，温度为25—250摄氏度)高压(针对X65管线钢，压力为5—20MPa)环境下具有应用前景。According to the above examples, it is shown that the electrode system of the present invention truly reflects the changes in electrochemical performance, indicating that the device operates at high temperature (for 304 stainless steel, the temperature is 25-250 degrees Celsius) and high pressure (for X65 pipeline steel, the pressure is 5-20MPa) It has application prospects in the environment.
以上对本发明进行了详细说明，但所述内容仅为本发明的较佳实施例，不能被认为用于限定本发明的实施范围。凡依本发明申请范围所作的均等变化与改进等，均应仍归属于本发明的专利涵盖范围之内。The present invention has been described in detail above, but the above contents are only preferred embodiments of the present invention and cannot be considered to limit the scope of implementation of the present invention. All equivalent changes and improvements made according to the scope of the application of the present invention should still belong to the scope of the patent of the present invention.
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